固相萃取-高效液相色谱法测定钙强化食品中的维生素D

以含有体积分数为20%的0.95 mol/L柠檬酸水溶液的二甲基亚砜作为维生素D的破壁溶液,利用Chromabond XTR固相萃取柱(14500 mg, 70 mL)对样品进行提取和净化,建立了测定钙强化食品中维生素D的固相萃取-高效液相色谱方法。方法的线性范围为0.1～100.0 μg/mL,线性相关系数为0.999。方法的定性检出限为0.01 μg/g,定量检出限为0.03 μg/g。低(0.1 μg/g)、中(0.5 μg/g)、高(1.0 μg/g)三个浓度水平的加标回收率分别为106.2%,99.5%和100.1%,相对标准偏差小于10%。

Determination of vitamin D in calcium fortified foods using solid-phase extraction-high performance liquid chromatography

A method for the determination of vitamin D in calcium fortified foods using solid-phase extraction-high performance liquid chromatography has been developed. The Chromabond XTR solid-phase extraction column (14,500 mg, 70 mL) was used to extract and clean-up the sample. The calibration curve of vitamin D showed good linearity in the range of 0.1-100.0 microg/mL with correlation coefficient of 0.999. The limit of qualification was 0.01 microg/g and the limit of quantification was 0.03 microg/g. The average recoveries at three spiking levels were 106.2%, 99.5%, 100.1%, and the relative standard deviations were lower than 10%.